CN113024284B - Method for preparing nitrogen-phosphorus-potassium compound fertilizer by fertilizer-grade phosphoric acid eutectic - Google Patents
Method for preparing nitrogen-phosphorus-potassium compound fertilizer by fertilizer-grade phosphoric acid eutectic Download PDFInfo
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- CN113024284B CN113024284B CN202011414387.7A CN202011414387A CN113024284B CN 113024284 B CN113024284 B CN 113024284B CN 202011414387 A CN202011414387 A CN 202011414387A CN 113024284 B CN113024284 B CN 113024284B
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- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05B—PHOSPHATIC FERTILISERS
- C05B11/00—Fertilisers produced by wet-treating or leaching raw materials either with acids in such amounts and concentrations as to yield solutions followed by neutralisation, or with alkaline lyes
- C05B11/04—Fertilisers produced by wet-treating or leaching raw materials either with acids in such amounts and concentrations as to yield solutions followed by neutralisation, or with alkaline lyes using mineral acid
- C05B11/10—Fertilisers produced by wet-treating or leaching raw materials either with acids in such amounts and concentrations as to yield solutions followed by neutralisation, or with alkaline lyes using mineral acid using orthophosphoric acid
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- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B7/00—Halogens; Halogen acids
- C01B7/01—Chlorine; Hydrogen chloride
- C01B7/03—Preparation from chlorides
- C01B7/035—Preparation of hydrogen chloride from chlorides
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Abstract
The invention provides a method for preparing a nitrogen-phosphorus-potassium proportion adjustable compound fertilizer by using fertilizer-grade phosphoric acid eutectic, which comprises the following steps: and (1) carrying out metathesis reaction. And (2) carrying out neutralization reaction. And (3) crystallizing and refining. And (4) filtering and drying. The invention has the beneficial effects that: the raw material cost is low, the recycling of the crystallization mother liquor and the recovery of the reaction by-product hydrogen chloride realize the zero emission of the whole process, and the high-efficiency utilization of the raw material is realized; the reaction is segmented, so that the conversion rate of potassium chloride in the reversible reaction is improved, and the problem of crop leaf burn caused by overhigh content of chloride ions in the fertilizer is solved; the content of nitrogen, phosphorus and potassium in the product is regulated and controlled by simply regulating and controlling the feeding ratio of the reaction raw materials, the controllable range is large, and different requirements of actual agricultural production on the fertilizer can be met.
Description
Technical Field
The invention belongs to the field of fertilizer preparation, and particularly relates to a method for preparing a compound fertilizer with adjustable nitrogen-phosphorus-potassium ratio by using fertilizer-grade phosphoric acid eutectic.
Background
The nitrogen, phosphorus and potassium are also called as fertilizer, which are essential nutrient elements for plant growth, and the nitrogen fertilizer, potassium fertilizer and phosphate fertilizer are the most important chemical fertilizers. China is a big agricultural country and a big world country for producing and using chemical fertilizers, however, most cultivated land soil in China has nitrogen content less than 0.2%, potassium-deficient soil reaches 4.5 hundred million acres, and phosphorus-deficient soil exceeds 10 hundred million acres, and with further development of agriculture, the demand and demand for fertilizers are increasingly increased, and the development of fertilizers suitable for complex soil conditions is particularly important. The potassium dihydrogen phosphate and the ammonium dihydrogen phosphate are high-quality phosphorus-potassium-phosphorus-nitrogen compound fertilizers, have high nutrient element content, obvious farming effect and low impurity content, and can be widely applied to agricultural irrigation and fertilization. The nitrogen, phosphorus and potassium ternary compound fertilizer can be developed by taking the two as raw materials, and different requirements in actual agricultural production can be met by regulating and controlling the nitrogen-phosphorus-potassium ratio in the product. At present, the nitrogen-phosphorus-potassium ternary compound fertilizer is mainly prepared by mixing two or three fertilizers, and a direct preparation process is not available.
Common potassium dihydrogen phosphate production methods include neutralization, direct, double decomposition, and electrolysis. The neutralization method mainly utilizes the reaction of phosphoric acid and alkaline substances such as potassium hydroxide, potassium carbonate and the like, and has the advantages of simple equipment, mature technology, high product purity, higher raw material cost and difficult application in agriculture. In contrast, the metathesis reaction has mild reaction conditions, simple operation and no pollution, but has the problem of higher chlorine content of the product. In the industry, the production method of ammonium dihydrogen phosphate is generally an ammonification method of phosphoric acid, the method has simple process and high production efficiency, but has the problems of difficult filtration of reaction products, poor crystal morphology and the like, and further crystallization optimization is needed.
Disclosure of Invention
In order to make up the problems in the production process of the prior ammonium dihydrogen phosphate and potassium dihydrogen phosphate, solve the recycling of waste acid in the phosphoric acid industry and also provide a direct preparation process for developing the nitrogen-phosphorus-potassium ternary compound fertilizer. The invention provides a preparation method of a ternary compound fertilizer of potassium dihydrogen phosphate and ammonium dihydrogen phosphate, wherein the nitrogen, phosphorus and potassium can be controlled.
The invention provides a method for preparing a nitrogen-phosphorus-potassium compound fertilizer by fertilizer-grade phosphoric acid eutectic, which comprises the following steps:
(1) Double decomposition reaction: adding fertilizer-grade phosphoric acid and potassium chloride into a reaction container, continuously supplementing water into the reactor before reaction, heating to 140-170 ℃ for reaction, introducing air, and blowing out HCl, wherein a first reaction mixture is obtained in the reaction container.
(2) And (3) neutralization reaction: and (2) cooling the first reaction mixture obtained in the step (1) to 30-60 ℃, adding ammonia water into the first reaction mixture, reacting to generate a solution of potassium dihydrogen phosphate and ammonium dihydrogen phosphate, and obtaining a second reaction mixture in the reaction container.
(3) And (3) crystallization and refining: and (3) transferring the second reaction mixture obtained in the step (2) into a crystallizer, heating to 60-80 ℃, cooling and crystallizing after the solid is dissolved, and performing eutectic crystallization to obtain potassium dihydrogen phosphate and ammonium dihydrogen phosphate crystals and a solution, wherein a solid-liquid mixture of the potassium dihydrogen phosphate and ammonium dihydrogen phosphate crystals and the solution is a third reaction mixture.
(4) And (3) filtering and drying: and (4) carrying out centrifugal separation on the third reaction mixture obtained in the step (3), drying a solid product obtained after centrifugation in a vacuum drying box, and recycling the liquid collected after centrifugation to the step (1).
The fertilizer grade phosphoric acid is phosphoric acid meeting the standard of HG T3826-2006, and the concentration of the phosphoric acid is 50-42%. The fertilizer grade phosphoric acid of the present invention also includes industrial phosphoric acid waste liquor meeting the above requirements in daily industrial production. Such phosphoric acids contain a variety of impurities, including oxides, metals, etc., that have unpredictable effects on metathesis and neutralization reactions. The invention overcomes the uncertainty and realizes the reutilization of the waste phosphoric acid in the preparation of the fertilizer.
Preferably, in step (1), the reactor is continuously replenished with water for the first 1 to 3 hours of the reaction.
In any of the above cases, it is preferable that the amount of water added per hour in the step (1) is 10 to 30% by mass of the raw material.
Any one of the above is preferred, the total time of step (1) is 2 to 5 hours.
Any one of the above is preferred, in the step (2), the concentration of the aqueous ammonia is 28 to 60% or 30 to 80%. Further, the concentration of ammonia water is preferably 28%, 30%, 40%, 50%, 60%, 70%, 80%.
Any one of the above is preferred, the feed of the raw materials potassium chloride, ammonia, fertilizer grade phosphoric acid satisfies n 1 +n 2 ≤n 3 Wherein n is 1 Is the mole number of KCl in the raw material potassium chloride, n 2 As NH in the raw material ammonia water 3 Mole number of (2), n 3 For H in fertilizer grade phosphoric acid 3 PO 4 The number of moles of (a). Preferably, n is 1 +n 2 ＝n 3 。
Any one of the above preferable ones is that the nitrogen-phosphorus-potassium ratio in the nitrogen-phosphorus-potassium compound fertilizer is adjustable, and the nitrogen-phosphorus-potassium ratio of the final product is regulated and controlled by controlling the feeding ratio of the reaction raw materials. The main reactions carried out by the invention comprise: h 3 PO 4 +KCl＝KH 2 PO 4 +HCl；H 3 PO 4 +NH 3 ＝NH 4 H 2 PO 4 N in the feed material 1 ：n 2 Determines the ratio of potassium element and nitrogen element in the final productFor example, the content of the phosphorus element of the compound fertilizer depends on n 1 +n 2 And/or n 3 The numerical value of (c).
Any one of the above is preferable, in the step (4), the drying time is 5 to 8 hours.
Any one of the above is preferred, in the step (4), the liquid collected after centrifugation is 5-40% phosphoric acid, and the reaction in the step (1) can be performed again after the phosphoric acid collected by centrifugation is mixed with fertilizer-grade phosphoric acid, thereby performing the steps (1) to (4) circularly. Step three the third reaction mixture also readily contains unreacted phosphoric acid.
The invention provides a method for preparing a compound fertilizer with adjustable nitrogen-phosphorus-potassium ratio by using fertilizer-grade phosphoric acid eutectic, which comprises the following steps:
(1) Double decomposition reaction: adding potassium chloride into the fertilizer phosphoric acid, and reacting to obtain a mixture of phosphoric acid and potassium dihydrogen phosphate. The blown gas is condensed and collected to obtain hydrochloric acid as a byproduct.
(2) And (3) neutralization reaction: adding strong ammonia water into the mixture, and reacting to obtain a mixture of potassium dihydrogen phosphate and ammonium dihydrogen phosphate.
(3) And (3) crystallization and refining: the mixture is transferred to a crystallizer, and the granularity appearance of the product is adjusted through the crystallization process, so that the purity is improved. The crystal grows well and the purity is high. The method for regulating and controlling the crystallization reaction comprises the steps of regulating the temperature reduction speed or the temperature rise speed, or changing the type of a solvent. Preferably, the temperature reduction in the cooling process is preferably to be reduced to 15 ℃ at the speed of 0.2 ℃/min, or an evaporative crystallization mode is adopted; water is preferably used as a solvent for controlling the crystallization process.
(4) And (3) filtering and drying: and after cooling crystallization is finished, filtering and drying the mixture to obtain the product compound fertilizer.
The invention discloses a method for preparing a compound fertilizer with adjustable nitrogen-phosphorus-potassium ratio by using fertilizer-grade phosphoric acid eutectic, which comprises the following steps:
the reaction of phosphoric acid and potassium chloride is reversible, and in order to ensure the reaction to be carried out, the invention designs that: the concentration of phosphoric acid in the fertilizer-grade phosphoric acid is higher, so that the reaction rate of the double decomposition reaction in the step (1) is improved; in the double decomposition reaction process of the step (1), phosphoric acid is always kept in excess and maintained at a high concentration, so that the conversion of potassium chloride is promoted, and the chlorine content in the product is reduced. In the step (1), the reaction product HCl is taken out by air and condensed with water vapor to form a byproduct hydrochloric acid, so that the forward direction of the reaction is promoted. And finally, performing neutralization reaction on the phosphoric acid and ammonia water to remove the residual phosphoric acid. The crystallization section further purifies the product, reduces the chloride ion content of the product, improves the granularity and the shape of the crystal product, reduces the product agglomeration, and has the function of readjusting the nitrogen-phosphorus-potassium ratio of the product.
The invention has the following beneficial effects:
1. the invention provides a method for preparing a compound fertilizer with adjustable nitrogen-phosphorus-potassium ratio by fertilizer-grade phosphoric acid eutectic. Fertilizer-grade phosphoric acid, potassium chloride, ammonia water and crystallization mother liquor are selected as raw materials, so that the cost of the raw materials is reduced. The recycling of the crystallization mother liquor and the recycling of the reaction byproduct hydrogen chloride also realize the zero emission of the whole process and realize the high-efficiency utilization of the raw materials.
2. The invention adopts the sectional reaction, preferentially converts the potassium chloride, greatly improves the conversion rate of the potassium chloride in the reversible reaction, and solves the problem of the burn of the leaves of the crops caused by overhigh content of chloride ions in the fertilizer.
3. The invention realizes the content regulation of nitrogen, phosphorus and potassium of the product by simply regulating the reaction raw material feeding ratio, has large controllable range and can meet different requirements of actual agricultural production on fertilizers.
The invention realizes the high-efficiency utilization of the industrial phosphoric acid waste liquid, the utilization rate of the phosphoric acid is more than 95 percent, the conversion rate of the potassium chloride is more than 99 percent by weight, the chlorine content of the product is small, the purity is high, the hydrogen chloride generated by the reaction is recycled to obtain the byproduct hydrochloric acid, and the zero emission of the whole process is realized. In addition, the nitrogen, phosphorus and potassium content of the final product can be regulated and controlled simply by adjusting the feeding ratio of the reaction raw materials, the controllable range is wide, and the produced ternary nitrogen, phosphorus and potassium compound fertilizer can meet different requirements in actual agricultural production.
Drawings
FIG. 1 is a schematic process flow diagram of the present invention.
FIG. 2 is a schematic view of a reaction apparatus of the present invention.
FIG. 3 is an XRD pattern of the products of embodiments 1-5 of the present invention.
Numbering in the drawings: 1. an air generator; 2. a three-neck flask; 3. oil bath pan; 4. a condenser tube; 5. a hydrochloric acid collecting bottle; and 6, naOH solution.
Detailed Description
The present invention will be more clearly and completely described in the following embodiments, but the described embodiments are only a part of the embodiments of the present invention, and not all of them. The examples are provided to aid understanding of the present invention and should not be construed to limit the scope of the present invention.
Example 1
64g of fertilizer grade phosphoric acid, 30g of crystallization mother liquor and 14.5g of potassium chloride were added to a three-necked flask, and magnetic stirring was turned on and an air generator was started. The oil bath was heated to 150 ℃ and 25g of water was added after 0.5 and 1.0 hour of reaction, respectively, for 1.5 hours. After the reaction is finished, the temperature of the system is reduced to 30 ℃, 26g of concentrated ammonia water with the mass fraction of 28-30% is slowly dripped, and the mixture is stirred for 0.5 hour. After the reaction is finished, collecting and storing a byproduct hydrochloric acid, transferring the prepared solid-liquid mixture of the potassium dihydrogen phosphate and the ammonium dihydrogen phosphate into a crystallizer, heating to 70 ℃, and cooling to 15 ℃ at the speed of 0.2 ℃/min after the solid is dissolved and clear. And (3) carrying out centrifugal separation on the solid-liquid mixture obtained by crystallization, and drying the solid phase in a vacuum drying oven at 70 ℃ to obtain the potassium dihydrogen phosphate and ammonium dihydrogen phosphate ternary compound fertilizer. The crystallization mother liquor (liquid obtained by centrifugation) was recovered as a raw material for metathesis reaction. And (3) the crystallization mother liquor is a liquid obtained after crystallization and filtration, namely the liquid collected after centrifugation in the step (4), and is circulated back to the step (1).
Example 2
64g of fertilizer grade phosphoric acid, 30g of crystallization mother liquor and 19g of potassium chloride were added to a three-necked flask, and magnetic stirring was turned on and an air generator was started. The oil bath was heated to 160 ℃ and 25g of water was added after reaction for 0.5,1.0 and 1.5 hours, respectively, for 2.0 hours. After the reaction is finished, the temperature of the system is reduced to 30 ℃, 22g of strong ammonia water with the mass concentration of 28-30% is slowly dripped, and the mixture is stirred for 0.5 hour. After the reaction is finished, collecting and storing a byproduct hydrochloric acid, transferring the prepared solid-liquid mixture of potassium dihydrogen phosphate and ammonium dihydrogen phosphate into a crystallizer, heating to 60 ℃, and cooling to 15 ℃ at the speed of 0.2 ℃/min after the solid is dissolved and clear. And (3) performing centrifugal separation on the solid-liquid mixture obtained by crystallization, and drying the solid phase in a vacuum drying oven at 70 ℃ to obtain the potassium dihydrogen phosphate and ammonium dihydrogen phosphate ternary compound fertilizer. The crystallization mother liquor is recovered as a raw material for metathesis reaction. And (3) the crystallization mother liquor is a liquid obtained after crystallization and filtration, namely the liquid collected after centrifugation in the step (4), and is circulated back to the step (1).
Example 3
64g of fertilizer grade phosphoric acid, 30g of crystallization mother liquor and 24g of potassium chloride are added into a three-neck flask, magnetic stirring is started, and an air generator is started. The oil bath was heated to 150 ℃ and 25g of water was added after reaction for 0.5,1.0,1.5 and 2.0 hours, respectively, for 2.5 hours. After the reaction is finished, the temperature of the system is reduced to 30 ℃, 18.5g of concentrated ammonia water with the mass concentration of 28-30% is slowly dripped, and the mixture is stirred for 0.5 hour. After the reaction is finished, collecting and storing byproduct hydrochloric acid, transferring the prepared solid-liquid mixture of potassium dihydrogen phosphate and ammonium dihydrogen phosphate into a crystallizer, heating to 70 ℃, and cooling to 15 ℃ at the speed of 0.2 ℃/min after the solid is dissolved and cleared. And (3) performing centrifugal separation on the solid-liquid mixture obtained by crystallization, and drying the solid phase in a vacuum drying oven at 70 ℃ to obtain the potassium dihydrogen phosphate and ammonium dihydrogen phosphate ternary compound fertilizer. The crystallization mother liquor is recovered as a raw material for metathesis reaction. And (5) the crystallization mother liquor is a liquid obtained after crystallization and filtration, namely the liquid collected after centrifugation in the step (4), and is circulated back to the step (1).
Example 4
64g of fertilizer grade phosphoric acid, 30g of crystallization mother liquor and 29g of potassium chloride were added to a three-necked flask, and magnetic stirring was turned on and an air generator was started. The oil bath was heated to 150 ℃ and 25g of water was added after reaction for 0.5,1.0,1.5 and 2.0 hours, respectively, for 2.5 hours. After the reaction is finished, the temperature of the system is reduced to 30 ℃, 15g of strong ammonia water with the mass concentration of 28-30% is slowly dripped, and the mixture is stirred for 0.5 hour. After the reaction is finished, collecting and storing a byproduct hydrochloric acid, transferring the prepared solid-liquid mixture of potassium dihydrogen phosphate and ammonium dihydrogen phosphate into a crystallizer, heating to 70 ℃, and cooling to 15 ℃ at the speed of 0.2 ℃/min after the solid is dissolved and clear. And (3) carrying out centrifugal separation on a solid-liquid mixture obtained by crystallization, and drying a solid phase in a vacuum drying oven at 70 ℃ to obtain the potassium dihydrogen phosphate and ammonium dihydrogen phosphate ternary compound fertilizer. The crystallization mother liquor is recovered as a raw material for metathesis reaction. And (3) the crystallization mother liquor is a liquid obtained after crystallization and filtration, namely the liquid collected after centrifugation in the step (4), and is circulated back to the step (1).
Example 5
64g of fertilizer grade phosphoric acid, 30g of crystallization mother liquor and 34g of potassium chloride were added to a three-necked flask, and magnetic stirring was turned on and an air generator was started. The oil bath was heated to 150 ℃ and 25g of water was added after reaction for 0.5,1.0,1.5,2.0 and 2.5 hours, respectively, for 3.0 hours. After the reaction is finished, the temperature of the system is reduced to 30 ℃, 11g of strong ammonia water with the mass concentration of 28-30% is slowly dripped, and the mixture is stirred for 0.5 hour. After the reaction is finished, collecting and storing a byproduct hydrochloric acid, transferring the prepared solid-liquid mixture of potassium dihydrogen phosphate and ammonium dihydrogen phosphate into a crystallizer, heating to 80 ℃, and cooling to 15 ℃ at the speed of 0.2 ℃/min after the solid is dissolved and clear. And (3) performing centrifugal separation on a solid-liquid mixture obtained by crystallization, and drying a solid phase in a vacuum drying oven at 70 ℃ to obtain the potassium dihydrogen phosphate and ammonium dihydrogen phosphate ternary compound fertilizer. The mother liquor of crystallization is recovered as a raw material for metathesis reaction. And (3) the crystallization mother liquor is a liquid obtained after crystallization and filtration, namely the liquid collected after centrifugation in the step (4), and is circulated back to the step (1).
The elemental content of the potassium dihydrogen phosphate and ammonium dihydrogen phosphate ternary compound fertilizer products obtained in the above embodiment examples 1-5 was measured, and the results are shown in table 1.
TABLE 1 Potassium chloride residual of Potassium dihydrogen phosphate and ammonium dihydrogen phosphate ternary Compound fertilizers products
Claims (5)
1. A method for preparing a nitrogen-phosphorus-potassium compound fertilizer by using fertilizer-grade phosphoric acid eutectic comprises the following steps:
(1) Double decomposition reaction: adding fertilizer-grade phosphoric acid into a reaction container, adding potassium chloride, continuously supplementing water into the reactor for the first 1-3 hours in the reaction, wherein the water supplementation amount per hour is 10-30% of the mass of the raw materials, then heating to 150 ℃ for reaction, simultaneously introducing air, blowing out HCl, reacting for 3.0 hours, and obtaining a first reaction mixture in the reaction container;
(2) And (3) neutralization reaction: cooling the first reaction mixture obtained in the step (1) to 30 ℃, adding ammonia water into the first reaction mixture, reacting to generate a solution of potassium dihydrogen phosphate and ammonium dihydrogen phosphate, and obtaining a second reaction mixture in the reaction container;
(3) And (3) crystallization and refining: transferring the second reaction mixture obtained in the step (2) into a crystallizer, heating to 60-80 ℃, cooling and crystallizing after dissolving the solid, and performing eutectic crystallization to obtain potassium dihydrogen phosphate and ammonium dihydrogen phosphate crystals and a solution, wherein a solid-liquid mixture of the potassium dihydrogen phosphate and the ammonium dihydrogen phosphate crystals and the solution is a third reaction mixture;
(4) And (3) filtering and drying: centrifuging the third reaction mixture obtained in the step (3), drying a solid product obtained after centrifugation in a vacuum drying oven, and circulating the liquid collected after centrifugation to the step (1);
in the step (3), the step of cooling and crystallizing is to transfer the second reaction mixture obtained in the step (2) into a crystallizer, heat the mixture to 60-80 ℃, and cool the mixture to 15 ℃ at a speed of 0.2 ℃/min after the solid is dissolved and clear;
in the step (1), the molar feeding ratio of potassium chloride to fertilizer-grade phosphoric acid to ammonia water is 0.7:1:0.3.
2. the method of claim 1, wherein in step (1), the blown HCl is condensed to collect hydrochloric acid as a byproduct.
3. The method of claim 1, wherein in step (2), the concentration of the aqueous ammonia is 28-30%.
4. The method of claim 1, wherein in step (4), the drying time is 5 to 8 hours.
5. The method of claim 1, wherein in step (4), the liquid collected after centrifugation is 5-40% phosphoric acid.
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| CN101734634A (en) * | 2008-11-04 | 2010-06-16 | 李海涛 | Method for producing monopotassium phosphate |
| CN101979311A (en) * | 2010-11-15 | 2011-02-23 | 中化重庆涪陵化工有限公司 | Method for producing industrial monopotassium phosphate and nitrogen, phosphorus and potassium compound fertilizer by using wet-process purified phosphoric acid as raw material through extraction |
| CN104386664B (en) * | 2014-10-30 | 2016-02-17 | 成都化工股份有限公司 | The method of ammonium potassium dihydrogen phosphate produced by fertilizer grade primary ammonium phosphate |
| CN107720713B (en) * | 2017-10-29 | 2020-11-20 | 贵阳开磷化肥有限公司 | Method for preparing ammonium dihydrogen phosphate and co-producing potassium dihydrogen phosphate by wet-process phosphoric acid |
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